HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86600020, compound → HCID 44474956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86600020 | HCID 86600020 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 44474956 | HCID 44474956 | — |
Reaction Steps
To a solution of the product from example 25 step a) (6.9 g) in THF (100 ml) was added borane-methylsulfide complex (4.4 ml) and the mixture heated under reflux for 2 hours. The mixture was carefully quenched by the addition of methanol (100 ml), evaporated to dryness and the residue taken up into methanol (100 ml) and acidified to pH 1-2 with concentrated hydrochloric acid. Heated under reflux for 30 mins then evaporated to dryness. The residue was triturated with ether to give a solid, which was collected by filtration, dissolved in water and the free base precipitated by the addition of aqueous sodium bicarbonate solution to give the subtitle compound (3.1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08143261B2 |
| Source dataset | uspto-grants-2012_03 |
| ORD ID | ord-7bf51de6565046ee8c2615df2077e922 |
| Source note | uspto-grants-2012_03 |